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\4m~ Designation:B 154 - 95

Standard Test Methodlor

Mercurous Nitrate Test f~)fCopper and Copper Alfoys 1
superscript epsiIon (E)indicates an editorial change sinee tbe last revision or reapproval.
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This standard is issued under tbe fixed designation B 154; tbe number immediate1y foUowing tbe designation indicates tbe year of original adoption or, in tbe case of revision, tbe year of 1ast revision. A number in parentbeses indicates tbe year of 1ast reapproval. A

This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 831 ofFederal Test Method Standard No. 151 b. Consult the DaD lndex of Specificmions and Standards for the specific year 01 issue that has been adopted by the Department of Delense.

1. Scope 1.1 Tbis test metbod describes tbe tecbnique for conducting tbe mercurous nitrate test for residual stress in wrougbt copper and cast or wrougbt copper-base alloy products. This test metbod is intended to cover tbe mercurous nitrate test of certain copper-alloy products supplied in accordance witb ASTM specifications prepared by Committee B-5. This test metbod is not intended to be used on assembled parts.
NOTEI-For any particularcopper alloy,referenceshouldbe made to the materialspecification.

1.2 Tbe values stated in SI units are to be regarded as tbe standard. Tbe values given in parentbeses are for information only. 1.3 This standard does not purport to address all of the safety concems, if any, associated with its use. lt is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applica"bility of regulatory limitations prior to use. For specific precautionary and bazard statements seeNotes 2, 3, 4, 5, and 6 and Sections 1, 4, 5, and 7.
NOTE 2: Warning-Mercury disposal. is a definite hea1th hazard in use and

4. Mercurous Nitrate Solution 4.1 Concentration- Tbe solution sball be an aqueous mercurous nitrate solution containing 10g of HgN03 and 10 mL of HN03 (sp gr 1.42)per litre of solution. 4.2 Preparation- Tbe aqueous mercurous nitrate solution shall be prepared by eitber of tbe followingprocedures, A or B. Used solutions may be replenisbed as described in 4.3. 4.2.1 Procedure A-Dissolve 11.4 g of HgN03.2H20 or 10.7 g of HgN03 .H20 in approximately 40 roL of distilled water acidified witb 10 mL of HN03 (sp gr 1.42). After tbe crystals are completely dissolved, dilute tbe solution witb distilled water to 1000 mL.
NOTE 3: Wamlng- The mercurous nitrate crystaIs are obtainable in both the monohydrate and dihydrate form and should be bandled with caution because of their highIy toxic effects. NOTE4: Caution-When weighing crystaIs, the weight ofthe water of crystallization should be taken into consideration. The mercurous nitrate crystals are photosensitive and when they have turned yellow are difficult to dissolve. NOTE5: Precaution-Care should be exercised when mixing chemicaJs. Mixing should only be done by qualified personnel using appropriate chemicallaboratory techniques.

2. Terminology 2.1 Dejinitions: 2.1.1 stress co"osion crack-spontaneous failure of metals by cracking under combined action of corrosion and stress, residual or applied. 2.1.2 residual stress-stresses tbat remain witbin a body as tbe result of plastic deformation or casting. 3. Significanceand Use 3.1 Tbis test metbod is an accelerated test for detecting tbe presence of residual (internal) stresseswhicb migbt result in failure of individual parts in storage or in service due to stress corrosion cracking. Tbis test metbod is not intended for assembliesunder applied stress. If used for tbat purpose it sball be for information only and not a cause for rejection of tbe assembly, its component parts, or tbe original mili producto
I This test metbod is under tbe jurisdiction of ASTM CommitteeB-5 on Copper and Copper Alloys and is tbe direct responsibility ofSubcommittee 805.06 on Metbods ofTest. Currentedition approved Sept. 10, 1995. Published November 1995. Origina1ly published as B 154 41 T. Last previous edition B 154 - 92.

4.2.2 Procedure B-Dissolve 76 g of mercury in 114 mL of diluted HN03 (1 part water to 1 part HN03) (sp gr 1.42). Carefully dilute witb distilled water to 1000 mL. This provides a concentration of 100 g of HgN03 after a sligbt 10ssdue 10 beating. Add tbe water in small portions while stirring to prevent local overdilution. Tbis gradual dilution, togetber witb tbe excess acid, will prevent precipitation of basic salts ofmercury. Dilute 100 mL oftbis solution (10 %) witb 7 mL ofHN03 (sp gr 1.42)and 893 mL ofwater.
NOTE 6: Warning-Mercury is a definite hea1th hazard and therefore equipment for the detection and removal of mercury vapor produced in volatilization is recommended. The use of rubber gloves in testing is advisable.

4.3 Replenishment of Solution- Tbe spent solution may be reclaimed by replenishing tbe mercurous nitrate solution, to a 1 % concentration, as follows: 4.3.1 Measure as accurately as possible in a small graduated cylinder 50 "mLof tbe spent HgN03 solution. 4.3.2 Transfer to an Erlenmeyer flask, and add 10 mL of HN03 (1 + 1). 4.3.3 Add slowly KMn04 solution (1 %) from a buret witb a constant shaking until tbere is an excess as indicated by tbe pink color, whicb persists for several minutes. 4.3.4 Add FeS04 crystalsuntil tbe solution, wben shaken, becomes clear. Tben titrate tbe solution witb 0.1 N KCNS solution to the appearance of a reddish brown color. Repeat

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4~ B 154
Replenlshment of Spent Mercurous Nltrate Solution to 1 '" Concentratlon NOTe-X= 111.1(1 - R) where:
R = fractlon of mercury remainlng in soIution (determined by titration). and X = number of millilltres of mercurous nitrate soIutlon (10 %) to be added to 1 L of spent mercurous nitrate solution to raise the concentration of mercurous nitrate to 1 %.

TABLE 1

R 0.10 0.12 0.14 0.16 0.18 0.20 0.22 0.24 0.26 0.28 0.30 0.32 0.34 0.36 0.38 0.40 0.42 0.44 0.46 0.48 0.50 0.52 0.54

X 100.0 97.8 95.5 93.3 91.1 88.9 86.7 84.4 82.2 80.0 77.8 75.5 73.3 71.1 68.9 66.7 64.4 62.2 60.0 57.8 55.6 53.3 51.1

R 0.56 0.58 0.60 0.62 0.64 0.66 0.68 0.70 0.72 0.74 0.76 0.78 0.80 0.82 0.84 0.86 0.88 0.90 0.92 0.94 0.96 0.98

X 48.9 46.7 44.4 42.2 40.0 37.8 35.6 33.3 31.1 28.9 26.7 24.4 22.2 20.0 17.8 15.6 13.3 11.1 8.9 6.7 4.4 2.2

5.2.5.1 Monitor the filtrate to assure it meets appropriate health safety standards, or is disposed of properly. 5.2.6 The precipitates should be collected and stored with the mercury contaminated test samples and sold to a licensed mercury disposal service. 6. Test Specimen 6.1 The test specimen shall be prescribed in the specification for the material being tested. In the event that a test specimen size is not prescribed in a given rod, wire, or tube specification, a full cross-section length of 6 in. (152 mm) shall be tested. 6.2 The presence of burrs on the test specimen may contribute to acceleration of stress corrosion cracking if not removed prior to the mercurous nitrate test. The burrs shall be removed by fine file or abrasive paper to facilitatethis test. 7. Procedure 7.1 Degrease the specimen in a suitable a1ka1ine degreasing solution or organic solventoIfnecessary, totally immerse the specimen in an aqueous solution of sulfuric acid (15 volume %) or nitric acid (40 volume %) until all oxides are completely removed from its surface or pickle in such solutions as may be prescribed in the specification for the material being tested. Remove the specimen from the. pickling solution and wash it immediately in running water. Drain the specimen free of excess water and totally immerse it at room temperature in the mercurous nitrate solution prepared in accordance with 4.2. Use at least 10 mL of mercurous nitrate solution per square inch of exposed surface of the test specimen. 7.2 After 30 min remove the specimen from the mercurous nitrate solution and wash it in running water. Wipe off any excess mercury from the surface of the specimen. Immediately examine it visually for cracks unless a time limitation is provided in the product specification. 7.2.1 Tested specimens are mercury contaminated and must be disposed of properly. They may not be included with retums for remelting or machined into producto 7.2.2 Make sure that rinse water and wiping material are monitored to ensure that they meet appropriate hea1thsafety standards, or are disposed of properly. 7.3 Do not reuse the solution unless it is replenished to 1 % in accordance with the procedure in 4.3. 8. Precision and Bias 8.1 No statement is made about the precision or bias of this test method since the procedure is directed at a subjective visual interpretation of condition of the specimen and its relation to an applicable product specification. 9. Keywords 9.1 mercurous nitrate; residual stress; stress corrosion

this procedure with 50 mL of a standard HgN03 solution (1 %). 4.3.5 The ratio, R. of the number of millilitres of KCNS solution required to titrate the spent solution, to the number of millilitres required to titrate the standard solution, determines the number of millilitres, X, of 10 % HgN03 in 3 % HN03 solution required to replenish 1 L of spent solution. Values of R and X for a litre volume are given in Table 1.

s. Hazards
5.1 Warning-Mercury is a definite health hazard in use and disposal. 5.2 Suggested Mercurous Nitrate Disposa/: 5.2.1 To mercurous nitrate solutions add sodium hydroxide to pH 10 to 11. 5.2.2 Filter precipitated mercury and other heavy metals. 5.2.3 Though the filtrate is low in free mercurous or mercuric ions, it must be further treated before disposal. 5.2.4 To each litre of filtrate, add two drops (0.1 cm3) of 24 % ammonium sulfide. 5.2.5 After the second fi1tering,the filtrate may be discarded.
NOTE 7-If heating is used in either of the previous procedures, the container should be covered with a watch glass to prevent 10ssof HN03

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41 B 154
The American Soclely wlth any Item mentioned patent rlghts, far Testlng and Materlals talees no pasltlon respectlng In thls standard. Users of thls standard are expressly of such rlghts, are entlrely the vaJldlty of any patent rlghts esserted In connectlon edvised that determlnatlon of the vaJldlty of any such

and the risk of Infrlngement

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Thls standard is subject to revislon at any time by the 'responslble technlcaJ commlttee and must be revlewed evlll)' five yeatS and if not revised, elther respproved ar wlthdrawn. Your comments are Invlted elther far revislon of thls standard ar far addltlonal standards and should be addressed lo ASTM Heedquarters, Your comments wlll rece/ve careful conslderatlon at a meeting of the responsible technlcal commlttee. whlch you may attend. If you feel that your comments have not recelved a falr haarlng you should malee your views known to the ASTM Commlttee on Standards, 1916 Race St., Phlladelphla, PA 19103. .

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